Development of a method for multielemental determination in water by EDXRF with radioisotopic source of 238Pu.

Camilo Fuentes Serrano; Juan Reinaldo Estevez Alvares; Alfredo Montero Alvarez; Ivan Pupo Gonzales; Zahily Herrero Fernandez; Dennys Leyva Bombuse; Piet Van Espen; Jossue Arteche Diaz; Lino Valcarcel Rojas; Jose Araujo Dos Santos Júnior

doi:10.15392/bjrs.v7i2A.627

Autores

Camilo Fuentes Serrano Center of Technological Applications and Nuclear Development
Juan Reinaldo Estevez Alvares Center of Technological Applications and Nuclear Development
Alfredo Montero Alvarez Center of Technological Applications and Nuclear Development
Ivan Pupo Gonzales Center of Technological Applications and Nuclear Development
Zahily Herrero Fernandez Center of Technological Applications and Nuclear Development
Dennys Leyva Bombuse Center of Technological Applications and Nuclear Development
Piet Van Espen University of Antwerp
Jossue Arteche Diaz Center of Technological Applications and Nuclear Development
Lino Valcarcel Rojas Center of Technological Applications and Nuclear Development
Jose Araujo Dos Santos Júnior Universidade Federal de Pernambuco

DOI:

https://doi.org/10.15392/bjrs.v7i2A.627

Palavras-chave:

multielemental determination, EDXRF, water

Resumo

A method for determination of Cr, Fe, Co, Ni, Cu, Zn, Hg and Pb in waters by Energy Dispersive X Ray Fluorescence (EDXRF) was implemented, using a radioisotopic source of ²³⁸Pu. For previous concentration was employed a procedure including a coprecipitation step with ammonium pyrrolidinedithiocarbamate (APDC) as quelant agent, the separation of the phases by filtration, the measurement of filter by EDXRF and quantification by a thin layer absolute method. Sensitivity curves for K and L lines were obtained respectively. The sensitivity for most elements was greater by an order of magnitude in the case of measurement with a source of ²³⁸Pu instead of ¹⁰⁹Cd, which means a considerable decrease in measurement times. The influence of the concentration in the precipitation efficiency was evaluated for each element. In all cases the recoveries are close to 100%, for this reason it can be affirmed that the method of determination of the studied elements is quantitative. Metrological parameters of the method such as trueness, precision, detection limit and uncertainty were calculated. A procedure to calculate the uncertainty of the method was elaborated; the most significant source of uncertainty for the thin layer EDXRF method is associated with the determination of instrumental sensitivities. The error associated with the determination, expressed as expanded uncertainty (in %), varied from 15.4% for low element concentrations (2.5-5 μg/L) to 5.4% for the higher concentration range (20-25 μg/L).

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Referências

Yagnentkovsky, N. Aplicación de técnicas de biorremediación para el tratamiento de residuos industriales con alto contenido de metales pesados (Doctoral dissertation, Facultad de Ciencias Exactas), (2011) http://sedici.unlp.edu.ar/bitstream/handle/10915/2706/Documento comple-to.pdf?sequence=1.

Tam N. F. Y., and Wong Y. S., “Spatial and temporal variations of heavy metal contamination in sediments of a mangrove swamp in Hong Kong,” Marine Pollution Bulletin, 31(4), pp. 254-261 (1995).

TUMA, Tratado Universal del Medio Ambiente. Madrid, España (1993).

Sereshti H., Heravi Y. E., and Samadi S., “Optimized ultrasound-assisted emulsification micro-extraction for simultaneous trace multielement determination of heavy metals in real water sam-ples by ICP-OES,” Talanta, 97, pp. 235-241 (2012).

Karimi M., Sereshti H., Khojeh V., and Samadi S., “Ligandless-ultrasound assisted emulsifica-tion microextraction followed by inductively coupled plasma optical emission spectrometry for simultaneous determination of heavy metals in water samples,” International Journal of Envi-ronmental Analytical Chemistry, 93(4), pp. 401-415 (2013).

Zhao L., Zhong S., Fang K., Qian Z., and Chen J., “Determination of cadmium (II), cobalt (II), nickel (II), lead (II), zinc (II), and copper (II) in water samples using dual-cloud point extraction and inductively coupled plasma emission spectrometry,” Journal of hazardous materials, 239, pp. 206-112 (2012).

Bauer G., Neouze M. A., Limbeck A., “Dispersed particle extraction—A new procedure for trace element enrichment from natural aqueous samples with subsequent ICP-OES analysis,” Ta-lanta, 103, pp. 145-152 (2013).

Yi Y. Z., Wu S. Y., Jiang S. J., and Sahayam A. C., “Cloud point extraction of Cr, Cu, Cd, and Pb from water samples and determination by electrothermal vaporization inductively coupled plasma mass spectrometry with isotope dilution,” Atomic Spectroscopy, 34(2), pp. 39-47 (2013).

Liao P. H., Jiang S. J., and Sahayam A. C., “Cloud point extraction combined with flow injec-tion vapor generation inductively coupled plasma mass spectrometry for preconcentration and determination of ultra trace Cd, Sb and Hg in water samples,” Journal of Analytical Atomic Spectrometry, 27(9), pp. 1518-1524 (2012).

Chandrasekaran K., Karunasagar D., and Arunachalam J., “Dispersive liquid–liquid micro ex-traction of boron as tetrafluoroborate ion (BF4−) from natural waters, wastewater and seawater samples and determination using a microflow nebulizer in inductively coupled plasma-quadrupole mass spectrometry,” Journal of Analytical Atomic Spectrometry, 28(1), pp. 142-149 (2013).

Kocot K., Zawisza B., and Sitko R., “Dispersive liquid–liquid microextraction using diethyl-dithiocarbamate as a chelating agent and the dried-spot technique for the determination of Fe, Co, Ni, Cu , Zn, Se and Pb by energy-dispersive X ray fluorescence spectrometry”, Spectro-chimica Acta Part B: Atomic Spectroscopy, 73, pp. 79-83 (2012).

Montero A., Estevez J.R., and Padilla R., “Heavy metal analysis of rainwaters by nuclear related techniques: Application of APDC precipitation and energy dispersive X-ray fluorescence,” Journal of Radioanalytical and Nuclear Chemistry, 245(3), pp. 485-489 (2000).

Leyva D., Estevez J.R., Montero A., Pupo I., “Separation and determination of selenium in wa-ter samples by the combination of APDC coprecipitation: X-ray fluorescence spectrometry,” Journal of Radioanalytical and Nuclear Chemistry, 291(3), pp. 699-705 (2012).

Poblete V., “Desarrollo de técnicas de preparación de muestras, para análisis por fluorescencia de rayos X,” Informe técnico de la Comisión Chilena de Energía Nuclear (CCHEN), Chile (1998).

Ellis A.T., Leyden D.E., Wegscheider W., Jablonski B.B. and Bodnar W.B., “Preconcentration methods for the determination of trace elements in water by x ray fluorescence spectrometry: Part 1. Response characteristics,” Analytica Chimica Acta, 142, pp. 73-87 (1982).

Orescanin V., Mikelic L., Lulic S., and Rubcic M., “Determination of Cr (III) and Cr (VI) in industrial and environmental liquid samples by EDXRF method,” Analytica Chimica acta, 527(2), pp. 125-129 (2004).

Quantitative X-Ray Analysis System (version 3.2), in Manual for QXAS/AXIL. 1995, IAEA: Vienna.

Torres E., Fuentes M., Greaves E.D., “SAX, software for the analysis of x-ray fluorescence spectra,” X-Ray Spectrometry, 27, pp.1661-165, (1998).

ISO 3696, Water for Analytical Laboratory Use, Specification and test method, (1987).

Holynska B., “Sampling and sample preparation in EDXRS,” X-Ray Spectrometry, 22, pp.192 (1993).

ISO 8466-1, Water Quality – Calibration and Evaluation of Analytical Methods and Estimation of Performance Characeristics, Part 1: Statistical evaluation of the linear calibration function (1990).

Currie L.A., “Limits for qualitative detection and quantitative determination. Application to radiochemistry,” Analytical Chemistry, 40(3), pp. 586-593 (1968).

Shakhashiro A., Regional PT on determination of trace elements in algae and water and radio-nuclides in soil and water, in Regional workshop on organization, evaluation and reporting of IC/PTs, RLA/2/013 and RLA/2/014-002. 2007, IAEA.

Cesur H., “Solid-phase extractions with freshly precipitated metal-diethyldithiocarbamates and atomic absorption spectrophotometric determination of cooper,” Journal of trace and microprobe techniques, 21(4), pp. 627-636 (2003).

Arain M., Khuhawar M. and Bhanger M., “Gas and liquid chromatography of metal chelates of pentamethylene dithiocarbamate,” Journal of Cromatography A, 973(1), pp. 235-241 (2002).

“National Primary Drinking Water Regulations,” https://www.epa.gov/ground-water-and-drinking-water/national-primary-drinking-water-regulations#Inorganic (2017).